Реакция #1427

Уравнение реакции

Potassium bromide

D-leucine

sodium nitrite

→

crude title product

(S)-2-Bromo-4-methylpentanoic acid

Растворители

sulfuric acid

Условия реакции

Обработка

1. 1
   Температураmaintaining the temperature between -10° and -5° C
2. 2
   workup.ADDITIONAfter addition
3. 3
   Температураwarmed to room temperature
4. 4
   workup.STIRRINGstirred for another hour
5. 5
   ЭкстракцияThe reaction mixture was then extracted twice with ether
6. 6
   Промывкаthe ether extracts were washed once with water
7. 7
   Сушкаdried (magnesium sulfate)
8. 8
   Фильтрацияfiltered
9. 9
   Другоеevaporated
10. 10
    Другоеto give 2.7 g

Методика

Potassium bromide (9.5 g., 80 mmol.) was added to a stirred solution of D-leucine (3.0 g., 23 mmol.) in 2.5N sulfuric acid (47 ml.) at room temperature. The reaction mixture was cooled to -10° C. and solid sodium nitrite (2.4 g., 34 mmol.) was added portionwise, maintaining the temperature between -10° and -5° C. After addition was complete, the reaction was stirred for 1 hour and then warmed to room temperature and stirred for another hour. The reaction mixture was then extracted twice with ether, the ether extracts were washed once with water, dried (magnesium sulfate), filtered and evaporated to give 2.7 g. of crude title product.

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